CN110229239A - A kind of microcrystalline cellulose and its production technology of high-bulk-density - Google Patents
A kind of microcrystalline cellulose and its production technology of high-bulk-density Download PDFInfo
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- CN110229239A CN110229239A CN201910692590.1A CN201910692590A CN110229239A CN 110229239 A CN110229239 A CN 110229239A CN 201910692590 A CN201910692590 A CN 201910692590A CN 110229239 A CN110229239 A CN 110229239A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/02—Oxycellulose; Hydrocellulose; Cellulosehydrate, e.g. microcrystalline cellulose
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Abstract
The present invention relates to microcrystalline cellulose fields, more particularly to the microcrystalline cellulose and its production technology of a kind of high-bulk-density, under the premise of microcrystalline cellulose molecular weight is identical, partial size is identical, increase its bulk density using physical method, the partial size D10 of microcrystalline cellulose produced is 10-30 μm, D50 is 45-70 μm, and D90 is 110-180 μm, bulk density 0.60-0.65g/cm3, greatly meet the differentiated demand in market.
Description
Technical field
The present invention relates to microcrystalline cellulose fields, and in particular to a kind of microcrystalline cellulose and its production work of high-bulk-density
Skill.
Background technique
Microcrystalline cellulose is usually used in the fields such as medicine, foods and cosmetics, and in pharmaceuticals industry, microcrystalline cellulose is usually used in
After preparation encounters liquid, moisture quickly enters inside the preparation containing microcrystalline cellulose disintegrating agent-as preparation, crystallite
The hydrogen bond of cellulose is broken at once, makes preparation disintegration release, so when the bulk density of microcrystalline cellulose is bigger, mobility
It is better, it is disintegrated faster.
With the development of science and technology, it is found that the size of microcrystalline cellulose bulk density is mainly fine with obtained crystallite
The molecular size range of dimension element has direct relation, related secondly with the particle size of microcrystalline cellulose, although utilizing above-mentioned two
The bulk density of part, the microcrystalline cellulose of existing technology production can generally reach 0.3-0.5g/cm3, but be difficult to meet market
On to the further demand of the microcrystalline cellulose of high-bulk-density.
Summary of the invention
The purpose of the present invention is to solve the above problem, under the premise of microcrystalline cellulose molecular weight is identical, partial size is identical,
Increase its bulk density by physical method, to increase the mobility of microcrystalline cellulose, meets the further demand in market.
To achieve the goals above, the present invention the following technical schemes are provided:
A kind of microcrystalline cellulose of high-bulk-density, bulk density 0.60-0.65g/cm3。
Prepare the production technology of the microcrystalline cellulose of above-mentioned high-bulk-density, comprising the following steps:
(1) it hydrolyzes: microcrystalline cellulose dissolving pulp being hydrolyzed into levelling off degree of polymerization 75-190 with acid；
(2) it filters: the microcrystalline cellulose dissolving pulp after hydrolysis is filtered, it is aobvious to be washed with water to filtrate for filter cake after filtering
Neutrality is washed with water again, and filter cake is spare；
(3) it mediates: filter cake being placed in kneader and is mediated；
(4) it is beaten: kneaded filter cake taking-up being placed in mashing tank, water is added and is beaten；
(5) drying and moulding: the slurry spray injection drying tower that will be prepared, the crystallite that spray drying obtains high-bulk-density are fine
Dimension element.
As the preferred embodiment of the invention, in step (1), the acid is 0.2mol/L-0.7mol/L hydrochloric acid, hydrolysis temperature
Degree is 90-110 degrees Celsius.
As the preferred embodiment of the invention, in step (1), microcrystalline cellulose dissolving pulp is hydrolyzed into levelling off degree of polymerization 150-
180。
As the preferred embodiment of the invention, in step (2), it is 70 μ s/cm-80 that filter cake, which is washed with water to filtrate conductivity,
μs/cm。
As the preferred embodiment of the invention, in step (3), the kneader includes to rotate forward paddle and counter-rotating rotors, wherein just
Turning paddle revolving speed is 37-50 revs/min, and counter-rotating rotors revolving speed is 21-38 revs/min, and the paddle and the structure of the reversion slurry of rotating forward is Z, W
Shape, kneading time are 20-27 minutes.
It is that 8%-32% is calculated purifying is added by filter cake solid content in step (4) as the preferred embodiment of the invention
Water, the revolving speed for being beaten tank is 350-650 revs/min, and beating time is 1-3 hours.
As the preferred embodiment of the invention, in step (5), the condition of the spray drying tower are as follows:
Inlet air temperature: 173-209 degrees Celsius,
Leaving air temp: 85-109 degrees Celsius,
Expect pump frequency: 29-33Hz,
Atomizer frequency: 29-36Hz.
The invention has the benefit that
It, can be in microcrystalline cellulose molecular weight is identical, partial size 1. by the improvement to microcrystalline cellulose manufacturing condition
Under the premise of identical, the higher microcrystalline cellulose of bulk density is prepared.
2. the bulk density of microcrystalline cellulose of the invention is 0.60-0.65g/cm3, there is very good mobility,
Disintegrating agent as preparation can be bigger increase preparation disintegrating property.
Specific embodiment
For the ease of the understanding of those skilled in the art, below with reference to embodiment, the present invention is further illustrated, real
The content for applying example is not limitation of the invention.
Embodiment one
A kind of microcrystalline cellulose and its production technology of high-bulk-density, comprising the following steps:
(1) it hydrolyzes: using 0.4mol/L dilute hydrochloric acid, it is in the case where reaction temperature is 110 degrees celsius, microcrystalline cellulose is molten
Pulp-water solution is solved to levelling off degree of polymerization 150；
(2) it filters: the microcrystalline cellulose dissolving pulp that levelling off degree of polymerization is 150 is filtered, filter cake is with drinking after filtering
Water washing is 72 μ s/cm to the aobvious neutrality of filtrate, then with purifying water washing to filtrate conductivity, and filter cake is spare；
(3) it mediates: filter cake being placed in kneader and is mediated；Rotating forward paddle and counter-rotating rotors in kneader select Z-shaped shape, setting
The revolving speed for rotating forward paddle is 37 revs/min, and counter-rotating rotors revolving speed is 22 revs/min, is mediated 20 minutes.
(4) it is beaten: kneaded filter cake taking-up being placed in mashing tank, is calculated by filter cake solid content 10% and purifying is added
The revolving speed of water, setting mashing tank is 400 revs/min, is beaten 1 hour；
(5) drying and moulding: the slurry spray injection drying tower that will be prepared, the inlet air temperature that spray drying tower is arranged is 170
Degree Celsius, leaving air temp is 90 degrees Celsius, and material pump frequency is 30HZ, and atomizer frequency is 31Hz.
The particle diameter distribution D10 that microcrystalline cellulose is made is 15 μm, and D50 is 49 μm, and D90 is 170 μm, and bulk density is
0.60g/m3。
Wherein:
Particle diameter distribution is detected using 3000 type laser granulometry of Malvern；
The measuring method of bulk density:
1. above-mentioned microcrystalline cellulose powder about 25mL is taken to be added in dry 50mL graduated cylinder；
2. rotating graduated cylinder, powder is made to sink naturally, top is in a horizontal state, and reads powder volume V；
3. powder is all poured out and weighs weight m, bulk density=m/V.
Embodiment two
A kind of microcrystalline cellulose and its production technology of high-bulk-density, comprising the following steps:
(1) it hydrolyzes: using 0.5mol/L dilute hydrochloric acid, it is in the case where reaction temperature is 100 degrees celsius, microcrystalline cellulose is molten
Solving pulp-water solution to levelling off degree of polymerization is 166；
(2) it filters: the microcrystalline cellulose dissolving pulp that levelling off degree of polymerization is 166 is filtered, filter cake is with drinking after filtering
Water washing is 75 μ s/cm to the aobvious neutrality of filtrate, then with purifying water washing to filtrate conductivity, and filter cake is spare；
(3) it mediates: filter cake being placed in kneader and is mediated；Rotating forward paddle and counter-rotating rotors in kneader select Z-shaped shape, setting
The revolving speed for rotating forward paddle is 42 revs/min, and counter-rotating rotors revolving speed is 36 revs/min, is mediated 25 minutes.
(4) it is beaten: kneaded filter cake taking-up being placed in mashing tank, is calculated by filter cake solid content 20% and purifying is added
The revolving speed of water, setting mashing tank is 510 revs/min, is beaten 1.5 hours；
(5) drying and moulding: the slurry spray injection drying tower that will be prepared, the inlet air temperature that spray drying tower is arranged is 200
Degree Celsius, leaving air temp is 98 degrees Celsius, and material pump frequency is 32Hz, and atomizer frequency is 35Hz.
The partial size D10 that microcrystalline cellulose is made is 20 μm, and D50 is 50 μm, and D90 is 175 μm, bulk density 0.65g/
m3。
Wherein:
Particle diameter distribution is detected using 3000 type laser granulometry of Malvern；
The measuring method of bulk density:
1. above-mentioned microcrystalline cellulose powder about 25mL is taken to be added in dry 50mL graduated cylinder；
2. rotating graduated cylinder, powder is made to sink naturally, top is in a horizontal state, and reads powder volume V；
3. powder is all poured out and weighs weight m, bulk density=m/V.
Embodiment three
A kind of microcrystalline cellulose and its production technology of high-bulk-density, comprising the following steps:
(1) it hydrolyzes: using 0.6mol/L dilute hydrochloric acid, it is in the case where reaction temperature is 95 degrees celsius, microcrystalline cellulose is molten
Solving pulp-water solution to levelling off degree of polymerization is 180；
(2) it filters: the microcrystalline cellulose dissolving pulp that levelling off degree of polymerization is 180 is filtered, filter cake is with drinking after filtering
Water washing is 70 μ s/cm to the aobvious neutrality of filtrate, then with purifying water washing to filtrate conductivity, and filter cake is spare；
(3) it mediates: filter cake being placed in kneader and is mediated；Rotating forward paddle and counter-rotating rotors in kneader select W-shape, setting
The revolving speed for rotating forward paddle is 50 revs/min, and counter-rotating rotors revolving speed is 38 revs/min, is mediated 30 minutes.
(4) it is beaten: kneaded filter cake taking-up is placed in mashing tank, calculate 25% addition by filter cake solid content and purify
The revolving speed of water, setting mashing tank is 600 revs/min, is beaten 2 hours；
(5) drying and moulding: the slurry spray injection drying tower that will be prepared, the inlet air temperature that spray drying tower is arranged is 180
Degree Celsius, leaving air temp is 85 degrees Celsius, and material pump frequency is 27HZ, and atomizer frequency is 27Hz.
The partial size D10 that microcrystalline cellulose is made is 18 μm, and D50 is 45 μm, and D90 is 160 μm, bulk density 0.62g/
m3。
Wherein:
Particle diameter distribution is detected using 3000 type laser granulometry of Malvern；
The measuring method of bulk density:
1. above-mentioned microcrystalline cellulose powder about 25mL is taken to be added in dry 50mL graduated cylinder；
2. rotating graduated cylinder, powder is made to sink naturally, top is in a horizontal state, and reads powder volume V；
3. powder is all poured out and weighs weight m, bulk density=m/V.
Above-described embodiment is the preferable implementation of the present invention, and in addition to this, the present invention can be existing with other way, not
Be detached from present inventive concept under the premise of it is any obviously replace it is within the scope of the present invention.
Claims (8)
1. a kind of microcrystalline cellulose of high-bulk-density, which is characterized in that the bulk density of the microcrystalline cellulose is 0.60-
0.65g/cm3。
2. prepare claim 1 described in a kind of production technology of the microcrystalline cellulose of high-bulk-density, which is characterized in that including with
Lower step:
(1) it hydrolyzes: microcrystalline cellulose dissolving pulp being hydrolyzed into levelling off degree of polymerization 75-190 with acid；
(2) filter: the microcrystalline cellulose dissolving pulp after hydrolysis be filtered, after filtering filter cake be washed with water to filtrate it is aobvious in
Property, it is washed with water again, filter cake is spare；
(3) it mediates: filter cake being placed in kneader and is mediated；
(4) it is beaten: kneaded filter cake taking-up being placed in mashing tank, water is added and is beaten；
(5) drying and moulding: the slurry spray injection drying tower that will be prepared, spray drying obtain the microcrystalline cellulose of high-bulk-density
Element.
3. technique according to claim 2, which is characterized in that in step (1), the acid is 0.2mol/L-0.7mol/L
Hydrochloric acid, hydrolysis temperature are 90-110 degrees Celsius.
4. technique according to claim 2, which is characterized in that in step (1), microcrystalline cellulose dissolving pulp is hydrolyzed into the limit
Degree of polymerization 150-180.
5. technique according to claim 2, which is characterized in that in step (2), filter cake is washed with water to filtrate conductivity and is
70μs/cm-80μs/cm。
6. technique according to claim 2, which is characterized in that in step (3), the kneader includes to rotate forward paddle and reversion
Paddle, wherein rotate forward paddle revolving speed be 37-50 revs/min, counter-rotating rotors revolving speed be 21-38 revs/min, it is described rotate forward paddle and it is described reversion slurry
Structure is Z, W-shape, and kneading time is 20-27 minutes.
7. technique according to claim 2, which is characterized in that be 8%-32% calculating by filter cake solid content in step (4)
Purified water is added, the revolving speed for being beaten tank is 350-650 revs/min, and beating time is 1-3 hours.
8. technique according to claim 2, which is characterized in that in step (5), the condition of the spray drying tower are as follows:
Inlet air temperature: 173-209 degrees Celsius,
Leaving air temp: 85-109 degrees Celsius,
Expect pump frequency: 29-33Hz,
Atomizer frequency: 29-36Hz.
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Cited By (3)
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| CN111333875A (en) * | 2020-04-13 | 2020-06-26 | 牡丹江霖润药用辅料有限责任公司 | Superfine high-performance microcrystalline cellulose product and preparation method thereof |
| CN113336863A (en) * | 2021-05-14 | 2021-09-03 | 珠海市东辰制药有限公司 | Microcrystalline cellulose and preparation method thereof |
| CN114028577A (en) * | 2021-10-20 | 2022-02-11 | 珠海市东辰制药有限公司 | Silicon dioxide pellet core and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111333875B (en) * | 2020-04-13 | 2023-02-07 | 牡丹江霖润药用辅料有限责任公司 | Superfine high-performance microcrystalline cellulose product and preparation method thereof |
| CN113336863A (en) * | 2021-05-14 | 2021-09-03 | 珠海市东辰制药有限公司 | Microcrystalline cellulose and preparation method thereof |
| CN114028577A (en) * | 2021-10-20 | 2022-02-11 | 珠海市东辰制药有限公司 | Silicon dioxide pellet core and preparation method thereof |
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